CN113939568A - 水性分散体和水性涂料组合物 - Google Patents
水性分散体和水性涂料组合物 Download PDFInfo
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- CN113939568A CN113939568A CN201980097317.2A CN201980097317A CN113939568A CN 113939568 A CN113939568 A CN 113939568A CN 201980097317 A CN201980097317 A CN 201980097317A CN 113939568 A CN113939568 A CN 113939568A
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- Prior art keywords
- aqueous dispersion
- emulsion polymer
- weight
- linear
- aqueous
- Prior art date
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- -1 siloxanes Chemical class 0.000 claims abstract description 54
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- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims description 3
- XASGNMMDXBCIHX-UHFFFAOYSA-N 2,4,6,8-tetrabutyl-2,4,6,8-tetrakis(ethenyl)-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound CCCC[Si]1(C=C)O[Si](CCCC)(C=C)O[Si](CCCC)(C=C)O[Si](CCCC)(C=C)O1 XASGNMMDXBCIHX-UHFFFAOYSA-N 0.000 claims description 2
- JMROMRCGLWRYBP-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetraethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound CC[Si]1(C=C)O[Si](CC)(C=C)O[Si](CC)(C=C)O[Si](CC)(C=C)O1 JMROMRCGLWRYBP-UHFFFAOYSA-N 0.000 claims description 2
- UWPCZMDZJREMAS-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetrahexyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound CCCCCC[Si]1(C=C)O[Si](CCCCCC)(C=C)O[Si](CCCCCC)(C=C)O[Si](CCCCCC)(C=C)O1 UWPCZMDZJREMAS-UHFFFAOYSA-N 0.000 claims description 2
- IUXIKQGXIZRSBF-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetrapropyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound CCC[Si]1(C=C)O[Si](CCC)(C=C)O[Si](CCC)(C=C)O[Si](CCC)(C=C)O1 IUXIKQGXIZRSBF-UHFFFAOYSA-N 0.000 claims description 2
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- 239000000654 additive Substances 0.000 description 5
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- 238000000113 differential scanning calorimetry Methods 0.000 description 5
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- 150000003254 radicals Chemical class 0.000 description 5
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229920002125 Sokalan® Polymers 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
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- 239000000243 solution Substances 0.000 description 4
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- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 3
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- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
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Abstract
提供了一种水性分散体,其包括:(a)乳液聚合物,(b)0.1%至5.5%的选自线性硅氧烷、环状硅氧烷及其混合物的不饱和硅氧烷,以及(c)零至3%的光交联剂,均是基于所述乳液聚合物的干重,以重量计的。还提供了一种制备所述水性分散体和包括其的水性涂料组合物的工艺。
Description
技术领域
本发明涉及一种水性分散体和一种包括其的水性涂料组合物。
背景技术
在外部涂料应用中,耐沾污性(DPUR)是使涂料能够在暴露于诸如阳光的元素时维持颜色和光泽的关键性质。诸如TiO2的无机颜料(用于油漆的常用白色颜料)在暴露于阳光时,可能会对涂料的耐久性产生不利影响。
将光交联剂掺入涂料中是涂料工业中用于改善DPUR性质的常用方法之一,这是因为其在阳光下能高效地生成自由基并且增加涂膜的表面硬度。涂料中最广泛使用的光交联剂包括二苯甲酮(BzP)、苯并三唑(BT)、三嗪(TA)和草酰苯胺(OA)的衍生物。然而,由这些光交联剂生成的自由基会导致聚合物降解,从而将损害长期耐久性。因此,期望提供一种适用于涂料应用的水性聚合物分散体,其提供具有改进的耐沾污性和长期耐久性的外部涂料,例如弹性建筑涂料。
发明内容
本发明提供了一种水性分散体,其包括乳液聚合物与特定量的式(I)的线性硅氧烷、式(II)的环状硅氧烷或所述线性硅氧烷和所述环状硅氧烷的混合物的混合物。本发明的水性分散体是存储稳定的。一种包括这样的水性分散体的水性涂料组合物可以提供由其制成的涂料,其具有改进的耐沾污性和长期耐久性,如由下面的示例部分中所述的测试方法确定的。
在第一方面,本发明是一种水性分散体,其包括:
(a)乳液聚合物,
(b)基于所述乳液聚合物的干重,按重量计0.1%至5.5%的硅氧烷,所述硅氧烷选自线性硅氧烷、环状硅氧烷及其混合物,其中所述线性硅氧烷具有下式(I),
其中R1和R4独立地选自-OH、-NH2、-NHR5和-NR5 2,其中每个R5独立地为C1-5烷基;每个R2独立地为具有一至三个双键的C2-10直链或支链烯基;每个R3独立地选自C1-6直链或支链烷基;R23为具有1至3个双键的C2-10直链或支链烯基或C1-6直链或支链烷基;m是2至40的整数;并且n为0至20的整数;
其中所述环状硅氧烷具有下式(II),
其中每个R6独立地选自氢和C1-6直链或支链烷基;每个R7独立地为具有一至三个双键的C2-10直链或支链烯基;并且z为1至20的整数;以及
(c)基于所述乳液聚合物的干重,按重量计0至3%的光交联剂。
在第二方面,本发明是一种制备第一方面所述的水性分散体的工艺。所述工艺包括:
混合乳液聚合物与基于所述乳液聚合物的干重,按重量计0.1%至5.5%的硅氧烷,所述硅氧烷选自线性硅氧烷、环状硅氧烷及其混合物;以及0至3%的光交联剂;
其中所述线性硅氧烷具有下式(I),
其中R1和R4独立地选自-OH、-NH2、-NHR5和-NR5 2,其中每个R5独立地为C1-5烷基;每个R2独立地为具有一至三个双键的C2-10直链或支链烯基;每个R3独立地为C1-6直链或支链烷基;R23为具有1至3个双键的C2-10直链或支链烯基或C1-6直链或支链烷基;m是2至40的整数;并且n为0至20的整数;
其中所述环状硅氧烷具有下式(II),
其中每个R6独立地选自氢和C1-6直链或支链烷基;每个R7独立地为具有一至三个双键的C2-10直链或支链烯基,并且z为1至20的整数。
在第三方面,本发明是一种水性涂料组合物,其包括第一方面所述的水性分散体以及颜料和/或增量剂。
具体实施方式
本文中的“水性”分散体是指分散在水性介质中的颗粒。本文中的“水介质”是指水和基于介质重按重量计零至30%的一种或多种水混溶性化合物,诸如,例如,醇、二醇、二醇醚、二醇酯等。
如本文所用的术语“丙烯酸”包括(甲基)丙烯酸、丙烯酸(甲基)烷基酯、(甲基)丙烯酰胺、(甲基)丙烯腈和其改性形式,例如丙烯酸(甲基)羟烷基酯。在整篇文件中,词语片段“(甲基)丙烯酰基”是指“甲基丙烯酰基”和“丙烯酰基”。例如,(甲基)丙烯酸是指甲基丙烯酸和丙烯酸两者,而(甲基)丙烯酸甲酯是指甲基丙烯酸甲酯和丙烯酸甲酯两者。
如本文所用,指定单体的术语结构单元(也称为聚合单元)是指在聚合之后所述单体的残余物。举例来说,甲基丙烯酸甲酯的结构单元如下说明:
本发明的水性分散体包括一种或多种选自线性硅氧烷、环状硅氧烷及其混合物的硅氧烷。水性分散体可以包括一种或多种具有下式(I)的线性硅氧烷,
其中R1和R4各自独立地选自-OH、-NH2、-NHR5和-NR5 2,其中每个R5独立地为C1-5烷基;每个R2独立地为具有一至三个双键(即,C=C键)的C2-10直链或支链烯基;每个R3独立地为C1-6直链或支链烷基;R23为具有1至3个双键的C2-10直链或支链烯基或C1-6直链或支链烷基;m是2至40的整数;并且n为0至20的整数;术语“烯基”在本文中是指通过从任何碳原子去除一个氢原子而由烯烃形成的一价烃基。R1和R4可以相同或不同。优选地,R1和R4独立地选自-OH和-NH2。优选地,R1和R4都是-OH。R2基团可以相同或不同。每个R2可以独立地具有2至10、2至8、2至7、2至6或2至5个碳原子。优选地,R2包含一个乙烯基。更优选地,R2是-CH=CH2;R3基团可以相同或不同。优选地,每个R3相同并且选自-CH3和-C2H5。m可以在2至40、3至30、4至20、4至16、5至15、6至12或8至12的范围内。n可以在0至20、0至10、0至6、0至4或0至3的范围内。线性硅氧烷可以是无规共聚物、嵌段共聚物或均聚物。
本发明的水性分散体可以包括一种或多种具有下式(I)的环状硅氧烷,
其中每个R6独立地选自氢和C1-6直链或支链烷基,诸如,例如,-CH3和-C2H5;每个R7独立地为具有一至三个双键(即,C=C键)的C2-10直链或支链烯基,优选为包含一个乙烯基,更优选地,R7为-CH=CH2;以及z为1至20、1至15、1至10、1至7、1至6、1至5或1至4的整数。R6基团可以相同或不同。优选地,每个R6相同并且选自-CH3和-C2H5。R7基团可以相同或不同。优选地,每个R7独立地选自乙烯基(-CH=CH2)、丙烯基、丁烯基和戊烯基。更优选地,每个R7独立地选自乙烯基和丙烯基。合适的环状硅氧烷可以包括,例如,四甲基四乙烯基环四硅氧烷、四乙基四乙烯基环四硅氧烷、四丙基四乙烯基环四硅氧烷、四丁基四乙烯基环四硅氧烷、四己基四乙烯基环四硅氧烷或其混合物。本发明的水性分散体可以包括一种或多种线性硅氧烷和一种或多种环状硅氧烷的组合。
基于乳液聚合物的干重,按重量计,水性分散体中的硅氧烷可以按0.1至5.5%,例如,0.1%或更多、0.2%或更多、0.3%或更多、0.4%或更多、0.5%或更多、0.6%或更多、0.7%或更多、0.8%或更多、0.9%或更多、1.0%或更多、1.1%或更多、1.2%或更多、1.3%或更多、1.4%或更多、或甚至1.5%或更多,以及同时,5.5%或更少、5.2%或更少、5%或更少、4.7%或更少、4.5%或更少、4.2%或更少、4%或更少、3.7%或更少、3.5%或更少、3.2%或更少、3%或更少、2.8%或更少、2.5%或更少、2.2%或更少、或甚至2%或更少的组合量存在。
本发明的水性分散体包括一种或多种乳液聚合物。乳液聚合物可以包括一种或多种单烯键不饱和离子单体的结构单元。在本文中,术语“离子单体”是指在pH=1-14之间带有离子电荷的单体。单烯键不饱和离子单体可以包括αβ-烯键不饱和羧酸和/或其酸酐,例如,(甲基)丙烯酸酐、马来酸酐或其混合物;亚磷酸单体和/或其盐,磺酸盐单体,诸如苯乙烯磺酸钠(SSS)和乙烯基磺酸钠(SVS)、丙烯酰胺基-2-甲基丙磺酸(AMPS)、丙烯酰胺基-2-甲基丙磺酸钠;或其混合物。合适的αβ-烯键不饱和羧酸可以包括例如,丙烯酸、甲基丙烯酸、巴豆酸、酰氧基丙酸、马来酸、富马酸、衣康酸或其混合物。亚磷酸单体可为醇的磷酸二氢酯,其中醇含有可聚合乙烯基或烯烃基团或经其取代。合适的单烯键不饱和亚磷酸单体及其盐可以包括(甲基)丙烯酸磷酸烷基酯,诸如(甲基)丙烯酸磷酸乙酯、(甲基)丙烯酸磷酸丙酯、(甲基)丙烯酸磷酸丁酯、其盐和其混合物;CH2=C(R)-C(O)-O-(RpO)p-P(O)(OH)2,其中R=H或CH3,Rp=烷基并且p=1-10,诸如均可购自苏威(Solvay)的SIPOMER PAM-100、SIPOMER PAM-200和SIPOMER PAM-300;(甲基)丙烯酸磷酸烷氧基酯,诸如(甲基)丙烯酸磷酸乙二醇酯、(甲基)丙烯酸磷酸二乙二醇酯、(甲基)丙烯酸磷酸三乙二醇酯、(甲基)丙烯酸磷酸丙二醇酯、(甲基)丙烯酸磷酸二丙二醇酯、(甲基)丙烯酸磷酸三丙二醇酯、其盐和其混合物。优选的单烯键不饱和离子单体选自由丙烯酸、甲基丙烯酸、苯乙烯磺酸钠、甲基丙烯酸磷酸乙酯(PEM)或其混合物。基于乳液聚合物的干重,按重量计,乳液聚合物可以包括0.05%或更多、0.1%或更多、0.3%或更多、0.5%或更多、或甚至1%或更多,以及同时,15%或更少、10%或更少、8%或更少、5%或更少、4%或更少、或甚至3%或更少的单烯键不饱和离子单体的结构单元。
可用于本发明的乳液聚合物还可以包括一种或多种单烯键不饱和非离子单体的结构单元。本文中“非离子单体”是指在pH=1-14之间不带有离子电荷的单体。单烯键不饱和非离子单体可以包括(甲基)丙烯酸的C1-C20、C1-C10或C1-C8-烷基酯。合适的单烯键不饱和非离子单体的示例包括丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸2-乙基己酯、丙烯酸癸酯、丙烯酸月桂酯、甲基丙烯酸甲酯、甲基丙烯酸丁酯、甲基丙烯酸异癸酯、甲基丙烯酸月桂酯、甲基丙烯酸羟乙酯、甲基丙烯酸羟丙酯,或其组合;(甲基)丙烯酰胺;(甲基)丙烯腈;脲基官能单体,诸如甲基丙烯酸羟乙基乙烯脲酯;甲基丙烯酸环烷基酯,诸如甲基丙烯酸环己基酯、丙烯酸甲基环己基酯、甲基丙烯酸异冰片酯、丙烯酸异冰片酯以及丙烯酸双环戊二烯酯;带有乙酰乙酸官能团的单体,诸如甲基丙烯酸乙酰乙酰氧基乙酯(AAEM);带有含羰基基团的单体,诸如二丙酮丙烯酰胺(DAAM);包括苯乙烯和被取代的苯乙烯的乙烯基芳香族单体,诸如α-甲基苯乙烯、对甲基苯乙烯、叔丁基苯乙烯、乙烯基甲苯,或其混合物;乙烯基三烷氧基硅烷,诸如乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷和乙烯基-三(2-甲氧基乙氧基)硅烷、乙烯基二甲基乙氧基硅烷、乙烯基甲基二乙氧基硅烷和(甲基)丙烯酰氧烷基三烷氧基硅烷,诸如(甲基)丙烯酰氧乙基三甲氧基硅烷和(甲基)丙烯酰氧丙基三甲氧基硅烷;丁二烯;α-烯烃,诸如乙烯、丙烯和1-癸烯;乙酸乙烯酯、丁酸乙烯酯、叔碳酸乙烯酯和其它乙烯酯;(甲基)丙烯酸缩水甘油基酯;或其组合。优选的单烯键不饱和非离子单体选自由以下组成的组:甲基丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸2-乙基己酯、苯乙烯及其混合物。基于乳液聚合物的干重,按重量计,乳液聚合物可以包括50%或更多、60%或更多、70%或更多、或甚至80%或更多,以及同时,99%或更少、98%或更少、95%或更少、90%或更少、或甚至85%或更少的单烯键不饱和离子单体的结构单元。
可用于本发明的乳液聚合物可任选地包含一种或多种多烯键式不饱和单体的结构单元,所述多烯键式不饱和单体包括二官能、三官能、四官能或更高多官能烯键式不饱和单体。合适的多烯键式不饱和单体可包括例如丁二烯、(甲基)丙烯酸烯丙酯、邻苯二甲酸二烯丙酯、二乙烯基苯、乙二醇二甲基丙烯酸酯、丁二醇二甲基丙烯酸酯或其混合物。基于乳液聚合物的重量,按重量计,乳液聚合物可以包括零至5%、0.05%至1%、或0.1%至0.5%的量的多烯键不饱和单体的结构单元。
可以选择上述单体的类型的水平以提供具有适合不同应用的玻璃化转变温度(Tg),例如,在-40℃至50℃、-35℃至35℃、-30℃至25℃或-25℃至10℃的范围内的乳液聚合物。Tg可以通过差示扫描量热法(DSC)测量,如下面的示例部分中所述。
水性分散体中的乳液聚合物颗粒可以具有50纳米(nm)至500nm、80至400nm、90至300nm或100至200nm的粒径。本文中的粒径是指Z平均大小,并且可以通过Brookhaven BI-90Plus粒径分析仪测量。
水性分散体中的乳液聚合物可以通过上述单体的乳液聚合制备。用于制备乳液聚合物的单体是用于形成乳液聚合物的结构单元的上述那些单体。用于制备乳液聚合物的单体的总重量浓度等于100%。基于用于制备聚合物的单体的总重量的每种单体的重量含量可以基本上与基于乳液聚合物的干重的这种单体的结构单元的重量含量相同。用于制备乳液聚合物的聚合技术是本领域公知的。单体混合物可以纯或于水中的乳液形式添加;或者在制备乳液聚合物的反应时段内以一次或多次添加或以线性或非线性的方式连续添加。适用于乳液聚合方法的温度可以低于100℃、在30℃到98℃的范围内或在50℃到95℃的范围内。可以利用使用上述单体的多级自由基聚合,其至少两个级按顺序形成,并且通常导致形成包括至少两种聚合物组合物的多级聚合物。
在制备乳液聚合物的聚合工艺中,可以使用一种或多种表面活性剂。可以在单体聚合之前或单体聚合期间或其组合中添加表面活性剂。聚合之后也可以添加一部分表面活性剂。这些表面活性剂可以包括阴离子和/或非离子表面活性剂。合适的表面活性剂的示例包括烷基、芳基或烷基芳基硫酸盐、磺酸盐或磷酸盐的碱金属盐或铵盐;烷基磺酸;磺基琥珀酸盐;脂肪酸;烯属不饱和表面活性剂单体;以及乙氧基化的醇或酚。在一些优选实施例中,使用非离子表面活性剂。市售的非离子表面活性剂可以包括,例如,TERGITOLTM 15-s-40、15-s-15、TMN-6和CA-90仲醇乙氧基化物、ECOSURFTM EH-9和EH-14仲醇乙氧基化物,以及TRITONTM X-405和HW 1000辛基苯酚乙氧基化物,其都可从陶氏化学公司获得(TERGITOL、ECOSURF和TRITON都是陶氏化学公司的商标)或其混合物。基于用于制备乳液聚合物的单体的总重量,按重量计,通常以0.1%至5%、0.15%至4%、0.2%至3%或0.2%至2%的量使用表面活性剂。
在制备乳液聚合物的聚合工艺中,可以使用一种或多种链转移剂。用于乳液聚合的合适的链转移剂的示例包括正十二烷基硫醇(nDDM)、以及3-巯基丙酸、3-巯基丙酸甲酯(MMP)、3-巯基丙酸丁酯(BMP)、苯硫酚、杜鹃花酸烷基硫醇、或其混合物。链转移剂可以控制乳液聚合物的分子量的有效量使用。优选地,基于用于制备乳液聚合物的单体的总重量,按重量计,链转移剂以0.01%或更多、0.05%或更多或甚至0.1%或更多,以及同时,2%或更少、1%或更少或甚至0.5%或更少的量使用。
在制备乳液聚合物的聚合过程中,可以使用自由基引发剂。所述聚合方法可以是热引发或氧化还原引发的乳液聚合。合适的自由基引发剂的实例包含过氧化氢、叔丁基过氧化氢、过氧化氢异丙苯、过硫酸铵和/或碱金属过硫酸盐、过硼酸钠、过磷酸和其盐;高锰酸钾和过二硫酸的铵或碱金属盐。基于单体的总重量,按重量计,自由基引发剂通常可以按0.1%至5%或0.3%至3%的水平使用。在聚合方法中可以使用包括上述引发剂和合适的还原剂的氧化还原体系。合适的还原剂的示例包括次硫酸氢钠甲醛、抗坏血酸、异抗坏血酸、含硫的酸的碱金属盐和铵盐,如亚硫酸钠、亚硫酸氢盐、硫代硫酸盐、次硫酸盐、硫化物、氢硫化物或连二亚硫酸盐、甲亚磺酸(formadinesulfinic acid)、丙酮亚硫酸氢盐、乙醇酸、羟基甲磺酸、乙醛酸水合物、乳酸、甘油酸、苹果酸、酒石酸和前述酸的盐。铁、铜、锰、银、铂、钒、镍、铬、钯或钴的金属盐可以用于催化氧化还原反应。可以任选地使用用于所述金属的螯合剂。
在完成乳液聚合物的聚合之后,可通过一种或多种碱作为中和剂将获得的乳液聚合物中和至例如至少6、6至10,或7至9的pH值。碱可导致乳液聚合物的离子基团或潜在离子基团的部分或完全中和。合适的碱的示例包括氨;碱金属或碱土金属化合物,诸如氢氧化钠、氢氧化钾、氢氧化钙、氧化锌、氧化镁、碳酸钠;伯胺、仲胺和叔胺,诸如三乙胺、乙胺、丙胺、单异丙胺、单丁胺、己胺、乙醇胺、二乙胺、二甲胺、三丁胺、三乙醇胺、二甲氧基乙胺、2-乙氧基乙胺、3-乙氧基丙胺、二甲基乙醇胺、二异丙醇胺、吗啉、乙二胺、2-二乙基氨基乙胺、2,3-二氨基丙烷、1,2-丙二胺、新戊二胺、二甲基氨基丙胺、六亚甲基二胺、4,9-二氧十二烷-1,12-二胺、聚乙烯亚胺或聚乙烯基胺;氢氧化铝;或其混合物。
本发明的水性分散体可以包括一种或多种非离子表面活性剂。合适的非离子表面活性剂包括在制备上面的乳液聚合物部分的聚合工艺中上述的那些。基于乳液聚合物的干重,按重量计,非离子表面活性剂可以按零至5%、0.1%至5%、0.15%至4%、0.2%至3%或0.2%至2%的量存在。
本发明的水性分散体还可以包括一种或多种光交联剂。可用于本发明的光交联剂可以包括二苯甲酮(BP)衍生物、苯并三唑(BTA)衍生物、酰基氧化膦、双酰基氧化膦或其混合物。
合适的二苯甲酮衍生物可以包括苯环中的一个或两个被取代的二苯甲酮衍生物,例如,二苯甲酮、4-甲基二苯甲酮、4-羟基二苯甲酮、4-氨基二苯甲酮、4-氯二苯甲酮、4-氢羧基二苯甲酮、4,4'-二甲基二苯甲酮、4,4'-二氯二苯甲酮、4-羧甲基二苯甲酮、3-硝基二苯甲酮或其混合物。优选的二苯甲酮衍生物是二苯甲酮或4-取代(对-)二苯甲酮。二苯甲酮是更优选的。
合适的苯并三唑衍生物可以包括例如,1,2-(2'-羟基苯基)苯并三唑,诸如2-(2'-羟基-5'-甲基苯基)苯并三唑、2-(3',5'-二叔丁基-2'-羟基苯基)苯并三唑、2-(5'-叔丁基-2'-羟基苯基)苯并三唑、2-(2'-羟基-5'-(1,1,3,3-四甲基丁基)苯基)苯并三唑、2-(3',5'-二叔丁基-2'-羟基苯基)-5-氯苯并三唑、2-(3'-叔丁基-2'-羟基-5'-甲基苯基)-5-氯苯并三唑、2-(3'-仲丁基-5'-叔丁基-2'-羟基苯基)苯并三唑、2-(2'-羟基-4'-辛氧基苯基)苯并三唑、2-(3',5'-二叔戊基-2'-羟基苯基)苯并三唑、2-(3',5'-双-(α,α-二甲基苄基)-2'-羟基苯基)-苯并三唑、2-(3'-叔丁基-2'-羟基-5'-(2-辛氧基羰基乙基)苯基)-5-氯苯并三唑、2-(3'-叔丁基-5'-[2-(2-乙基-己基-氧基)羰基乙基]-2'-羟基苯基)-5-氯苯并三唑、2-(3'-叔丁基-2'-羟基-5'-(2-甲氧羰基乙基)苯基)-5-氯苯并三唑、2-(3'-叔丁基-2'-羟基-5'-(2-甲氧基羰基乙基)苯基)苯并三唑、2-(3'-叔丁基-2'-羟基-5'-(2-辛氧基-羰基乙基)苯基)苯并三唑、2-(3'-叔丁基-5'-[2-(2-乙基己氧基)羰基乙基]-2'-羟基苯基)苯并三唑、2-(3'-十二烷基-2'-羟基-5'-甲基苯基)苯并三唑和2-(3'-叔丁基-2'-羟基-5'-(2-异辛氧基羰基乙基)苯基苯并三唑的混合物以及2,2'-亚甲基-双[4-(1,1,3,3-四甲基丁基)-6-苯并三唑-2-基-苯酚];2-[3'-叔丁基-5'-(2-甲氧基羰基乙基)-2'-羟基-苯基]-苯并三唑与聚乙二醇300的酯交换产物;[R-CH2-CH2-COO(CH2)3]2,其中R=3'-叔丁基-4'-羟基-5'-2H-苯并三唑-2-基-苯基或其混合物。
合适的酰基氧化膦可以包括例如,2,6-二甲基苯甲酰基二苯基氧化膦、2,4,6-三甲基苯甲酰基二苯基氧化膦、双(2,4,6-三甲基苯甲酰基)苯基氧化膦、2,6-二氯苯甲酰基-二苯基氧化膦和2,6-二甲氧基苯甲酰基二苯基氧化膦,或其混合物。
合适的双酰基氧化膦可以包括例如,双(2,6-二甲氧基苯甲酰基)-2,4,4-三甲基戊基氧化膦、双(2,6-二甲基苯甲酰基)-2,4,4-三甲基戊基氧化膦、双(2,4,6-三甲基苯甲酰基)-2,4,4-三甲基戊基氧化膦和双(2,6-二氯苯甲酰基)-2,4,4-三甲基戊基氧化膦,或其混合物。
基于乳液聚合物的干重,按重量计,可用于本发明的光交联剂可以按零至3%,例如,0.01%或更多、0.02%或更多、0.03%或更多、0.04%或更多、0.05%或更多、0.06%或更多、0.07%或更多、0.08%或更多、0.09%或更多、0.10%或更多、0.12%或更多、0.15%或更多、0.18%或更多或甚至0.20%或更多,并且同时,3.0%或更少、2.8%或更少、2.5%或更少、2.2%或更少、2.0%或更少、1.8%或更少、1.5%或更少、1.4%或更少、1.3%或更少、1.2%或更少、1.1%或更少、1.0%或更少、0.9%或更少、0.8%或更少、0.7%或更少、0.6%或更少或甚至0.5%或更少的量存在。在一些实施例中,本发明的水性分散体基本上不含光交联剂(即,小于0.01%,优选为零),同时仍实现了令人满意的DPUR性质。
本发明的水性分散体还包括水。基于水性分散体的总重量,按重量计,水的浓度可以为30%至90%或40%至80%。本发明的水性分散体可以用于许多应用,包括例如,木器涂料、建筑涂料、金属涂料和路标漆。
本发明的水性分散体可以通过混合乳液聚合物与硅氧烷,以及可选地,光交联剂、非离子表面活性剂和其他可选的组分来制备。本发明还涉及一种通过混合乳液聚合物与硅氧烷,以及可选地,光交联剂来制备水性分散体的工艺。本发明的水性分散体是一种稳定的水性分散体,其在50℃下存储28天之后没有显著的相分离(即,没有显著的分层),如根据上述测试方法确定的。
本发明还涉及一种包括本发明的水性分散体的水性涂料组合物。基于水性涂料组合物的总干重,按重量计,水性涂料组合物可以包括20%至99.5%、30%至98%或35%至95%的水性聚合物分散体。
本发明的水性涂料组合物还可以包括颜料。本文中的“颜料”是指能够实质上有助于涂料的不透明性或遮盖能力的颗粒状无机材料。这类材料的折射率通常大于1.8。无机颜料可以包括例如二氧化钛(TiO2)、氧化锌、氧化铁、硫化锌、硫酸钡、碳酸钡或其混合物。在优选实施例中,本发明中所用的颜料是TiO2。TiO2通常以两种晶体形式存在,即锐钛矿和金红石。TiO2还可以以浓缩分散体的形式获得。水性涂料组合物还可以包括一种或多种增量剂。本文中的“增量剂”是指折射率小于或等于1.8并且大于1.3的颗粒无机材料。合适的增量剂的示例包括碳酸钙、粘土、硫酸钙、铝硅酸盐、硅酸盐、沸石、云母、硅藻土、实心或中空玻璃、瓷珠、霞石正长岩、长石、硅藻土、煅烧硅藻土、滑石(水合硅酸镁)、二氧化硅、氧化铝、高岭土、叶蜡石、珍珠岩、重晶石、硅灰石、不透明聚合物(例如可购自陶氏化学公司的ROPAQUETM Ultra E(ROPAQUE为陶氏化学公司的商标)或其混合物。水性涂料组合物可以具有8%至70%、12%至60%或15%至55%的颜料体积浓度(PVC)。PVC可以由下列等式确定:PVC=[体积(颜料+增量剂)/体积(颜料+增量剂+粘合剂)]×100%。
本发明的水性涂料组合物还可以包括一种或多种消泡剂。本文中“消泡剂”是指减少泡沫并且阻止泡沫形成的化学添加剂。消泡剂可为硅酮基消泡剂、矿物油基消泡剂、环氧乙烷/环氧丙烷基消泡剂、聚丙烯酸烷基酯或其混合物。合适的可商购的消泡剂包括例如均购自迪高(TEGO)的TEGO Airex 902W和TEGO Foamex 1488聚醚硅氧烷共聚物乳液、可购自毕克(BYK)的BYK-024硅酮消泡剂,或其混合物。基于水性涂料组合物的总干重,按重量计,消泡剂可以按零至2%、0.1%至1.5%或0.2%至1%的量存在。
本发明的水性涂料组合物还可以包括一种或多种增稠剂。增稠剂可以包括聚乙烯醇(PVA)、粘土材料、酸衍生物、酸共聚物、氨基甲酸酯缔合增稠剂(UAT)、聚醚脲聚氨酯(PEUPU)、聚醚聚氨酯(PEPU)或它们的混合物。合适的增稠剂的示例包括碱可溶胀的乳液(ASE),如钠或铵中和的丙烯酸聚合物;疏水改性的碱可溶胀的乳液(HASE),如疏水改性的丙烯酸共聚物;缔合增稠剂,如疏水改性的乙氧基化氨基甲酸酯(HEUR);和纤维素增稠剂,如甲基纤维素醚、羟甲基纤维素(HMC)、羟乙基纤维素(HEC)、疏水性改质的羟乙基纤维素(HMHEC)、羧甲基纤维素钠(SCMC)、羧甲基2-羟乙基纤维素钠、2-羟丙基甲基纤维素、2-羟乙基甲基纤维素、2-羟丁基甲基纤维素、2-羟乙基乙基纤维素和2-羟丙基纤维素。优选地,增稠剂为疏水改性的羟乙基纤维素(HMHEC)。基于水性涂料组合物的总干重,按重量计,增稠剂的浓度可以是零至4%、0.2%至3%或0.4%至2%的量。
本发明的水性涂料组合物可以进一步包括一种或多种润湿剂。本文中的“润湿剂”是指降低涂料组合物的表面张力,从而使涂料组合物更容易跨基材表面扩散或渗透基材表面的化学添加剂。润湿剂可以是阴离子型、两性离子型或非离子型聚羧酸盐。基于水性涂料组合物的总干重,按重量计,湿润剂可以按零至3%、0.1%至2.5%或0.2%至2%的量存在。
本发明的水性涂料组合物可另外包含一种或多种分散剂。分散剂可以包括非离子、阴离子和阳离子分散剂,诸如具有适合分子量的多元酸、2-氨基-2-甲基-1-丙醇(AMP)、二甲基氨基乙醇(DMAE)、三聚磷酸钾(KTPP)、聚磷酸三钠(TSPP)、柠檬酸和其它羧酸。使用的多元酸可以包括基于多元羧酸的均聚物和共聚物(例如,重均分子量在1,000至小于50,000的范围内,如通过凝胶渗透色谱法(GPC)测量的),包括已经疏水或亲水改性的那些,例如,聚丙烯酸或聚甲基丙烯酸或马来酸酐与各种单体,诸如苯乙烯、丙烯酸酯或甲基丙烯酸酯、二异丁烯和其它亲水或疏水共聚单体;其盐;或其混合物。基于水性涂料组合物的总干重,按重量计,分散剂可以按零至3%、0.1%至2%、0.2%至1.5%或0.3%至1.2%的量存在。
本发明的水性涂料组合物可以进一步包括一种或多种聚结剂。本文中的“聚结剂”是指在环境条件下使聚合物颗粒融合成连续膜的缓慢蒸发溶剂。合适的聚结剂的示例包括2-正丁氧基乙醇、二丙二醇正丁醚、丙二醇正丁醚、二丙二醇甲醚、丙二醇甲醚、丙二醇正丙醚、二乙二醇单丁醚、乙二醇单丁醚、乙二醇单己醚、三乙二醇单丁醚、二丙二醇正丙醚、正丁醚或其混合物。优选的聚结剂包括二丙二醇正丁醚、乙二醇单丁醚、二乙二醇单丁醚、正丁醚或其混合物。基于水性涂料组合物的总干重,按重量计,聚结剂可以按零至30%、0.1%至20%或0.5%至15%的量存在。
除了上述组分之外,本发明的水性涂料组合物还可以包括下列添加剂中的任何一种或组合:缓冲剂、中和剂、防冻剂、保湿剂、防霉剂、杀生物剂、防结皮剂、着色剂、流动剂、抗氧化剂、增塑剂、流平剂、触变剂、增粘剂和研磨媒剂。基于水性涂料组合物的干重,按重量计,这些添加剂可以按零至5%、0.1%至4%、或0.5%至3%的组合量存在。
本发明的水性涂料组合物可以通过混合水性分散体与其他可选组分,例如,如上所述的颜料和/或增量剂来制备。可以按任何顺序混合水性涂料组合物中的组分,以提供本发明的水性涂料组合物。还可以将上述任选的组分中的任一种在混合期间或之前添加至所述组合物,以形成所述水性涂料组合物。当水性涂料组合物包括颜料和/或增量剂时,即,颜料配制物、颜料和/或增量剂优选地与作为分散体的水性聚合物分散体混合,以形成颜料和/或增量剂的浆液。然后可以将获得的混合物在研磨或碾磨装置中进行剪切,如颜料分散领域中众所周知的那样。这样的研磨或碾磨装置包括辊磨机、球磨机、珠磨机、磨碎机,并且包括混合物在其中连续再循环的磨机。混合物的剪切继续进行足够的时间以分散颜料。足以分散颜料的时间通常取决于颜料和作为分散体的水性聚合物分散体的性质,以及所使用的研磨或碾磨装置,并且将由熟练的从业者确定。
本发明还涉及一种使用本发明的水性涂料组合物的工艺。该工艺可以包括以下步骤:将水性涂料组合物涂施至基材,和干燥或允许干燥所涂施的水性涂料组合物。本发明还涉及在基材上生产涂层的方法,其包括:将本发明的水性涂料组合物涂施在基材上,并且干燥或使水性涂料组合物干燥以形成如上所述的具有改进的耐沾污性(DPUR)的涂料。此处“改进的DPUR”表示本发明的水性涂料组合物提供了具有比不存在上述硅氧烷的相同涂料组合物(“常规涂料组合物”)更小的ΔY值,例如,至少比常规涂料组合物低1.4%、至少低2%、至少低4%、至少低5%或至少低6%的ΔY值的涂料。本发明的水性涂料组合物还可以提供比常规涂料组合物更好的耐久性,例如,如在室外暴露至少9个月后比常规涂料组合物低至少3的ΔE值所示。DPUR和耐久性性质可以根据在下面的示例部分中所述的测试方法测量。
本发明的水性涂料组合物可以涂施并粘附至各种基材上。合适的基材的示例包括木材、金属、塑料、泡沫、石头、弹性基材、玻璃、织品、混凝土或水泥质基材。优选地包含颜料的涂料组合物适合于各种应用,诸如海洋和防护涂料、汽车涂料、交通漆、外墙外保温装饰系统(EIFS)、屋面胶泥、木材涂料、卷材涂料、塑料涂料、粉末涂料、罐头涂料、建筑涂料和土木工程涂料。涂料组合物特别适合用于建筑涂料。
本发明的水性涂料组合物可以通过包括刷涂、浸涂、辊涂和喷涂在内的现有方法涂施至基材。水性组合物优选地通过喷涂而涂施。可使用标准喷涂技术和装备进行喷涂,诸如空气雾化喷涂、空气喷涂、无空气喷涂、高容量低压喷涂和静电喷涂(如静电喷涂)以及手动或自动方法。在将本发明的涂料组合物涂施至基材上后,可在室温(20℃-25℃)下或在高温(例如,35℃至80℃)下干燥涂料组合物或允许干燥涂料组合物,以形成膜(即,涂层)。
示例
现在将在以下示例中描述本发明的一些实施例,除非另外说明,否则其中所有份数和百分比均以重量计。
四(二甲基乙烯基硅氧基)硅烷(QMVi 4)可购自陶氏化学公司。
可购自陶氏化学公司的环状甲基乙烯基硅氧烷(环状DViMe 4)是四甲基四乙烯基环四硅氧烷。
可购自国药集团化学试剂有限公司二苯甲酮(BzP)具有以下结构:
在示例中使用以下标准分析设备和方法。
油漆面板的制备
根据以下程序制备油漆面板:
(i)将具有下表3所示组成的外部底漆通过湿荷载为120g/m2的辊涂施至水泥面板,并且在恒温室(CTR)(25℃以及50%的相对湿度(RH))中固化2小时;
(ii)将待测试的涂料组合物以每平方米200克(g/m2)的湿荷载刷涂至从步骤(i)获得的上述涂有底漆的面板上,并且随后在CTR(25℃和50%的RH)中固化2小时;
(iii)将待测试的涂料组合物的第二层以200g/m2的湿荷载刷涂至从步骤(ii)获得的面板上;以及
(iv)在根据下面的程序对白色油漆进行以下的实验室DPUR和室外DPUR测试以及对蓝色油漆进行耐久性测试之前,在CTR(25℃和50%的RH)中将得到的油漆面板固化7天。
实验室耐沾污性(DPUR)测试
基于下述的白色涂料组合物,根据上述步骤(i)至(iv)制备白色油漆面板。根据GB/T 9780-2013(建筑涂料涂层耐沾污性试验方法)评估油漆面板。用紫外光(波长:360nm)照射面板4小时,并且然后测量初始反射率值,其被表示为Y*初始。配制灰分(0.7±0.1g,52.6重量%,中国优图仪器公司)与水混合,并且然后涂刷在油漆面板上。将面板在CTR(25℃和50%的RH)中干燥2小时,并且然后用水以最大流量均匀地洗涤1分钟以及干燥过夜。然后,涂施灰分,干燥2小时,洗去灰分以及在CTR中干燥过夜,构成一个循环,并且重复5次。测量最终的反射率值,其被表示为Y*最终。
室外DPUR测试
基于下述的白色涂料组合物,根据上述步骤(i)至(iv)制备白色油漆面板。测量油漆面板的初始Y*值。然后这些白色油漆面板进行室外暴露。暴露方向为45°南角。在暴露9个月之后,观察面板的外观变化并且将最终Y*值记录为Y*最终。
对于上述实验室DPUR和室外DPUR测试而言,Y*初始值和Y*最终值由光谱导向的球形光泽便携式分光光度计(BYK-Gardner)测量。根据以下等式计算分别用于实验室DPUR和室外DPUR测试的被表示为ΔY(%)的反射Y的变化率:
ΔY(%)=(Y*初始–Y*最终)/Y*初始×100%
ΔY值越小,DPUR的性质越好。
耐久性测试
基于下述的蓝色涂料组合物,根据上述步骤(i)至(iv)制备蓝色油漆面板。面板的初始L*初始,a*初始和b*初始值由光谱导向的球形光泽便携式分光光度计(BYK-Gardner)测量并且被分别记录为L*初始,a*初始和b*初始。然后这些面板进行室外暴露。暴露方向为45°南角。在暴露9个月之后,观察面板的外观变化并且将最终L*,a*和b*值记录为L*最终,a*最终和b*最终。根据下式计算表示样品的耐久性的ΔE值,
机械性质
根据JG/T 172-2005弹性建筑涂料标准,通过使用AI-7000M通用测试来测量包括断裂伸长率和拉伸强度的机械性质。使用涂施器将要测试的涂料组合物涂施至剥离纸以形成湿膜厚度为1,500μm的第一层。24小时后,将涂料组合物的第二层涂施在湿膜厚度为1,500μm的第一层上。再过24小时后,将涂料组合物的第三层涂施在湿膜厚度为1,000μm的第二层上。将涂布纸在CTR(25℃,50%的RH)中干燥2天,并且随后放入80℃的烘箱中4天。将涂布纸从烘箱取出,并且随后在CTR(25℃,50%的RH)中保持2天。将得到的涂覆膜从剥离纸剥离并且由特殊刀模切成哑铃形。由在1.0±0.2mm范围内的干膜厚度选择膜。然后评估涂膜的断裂伸长率和室温下最大拉伸强度,其分别被表示为“RT伸长率”和“RT拉伸强度”。对于低温机械性能测试而言,测试前将干膜置于-10℃的环境箱中30分钟,并且测试的断裂伸长率和最大拉伸强度被分别表示为“LT伸长率”和“LT拉伸强度”。
水性分散体的稳定性
首先将乙烯基硅氧烷与粘合剂以预定剂量在室温下以400转/分钟(rpm)混合20分钟以形成水性分散体。将20ml所得水性分散体立即倒入直径为1.4厘米(cm)的试管中。管中水性分散体的高度为13.0cm,其被表示为“原始高度”。将试管存储在50℃的烘箱中28天。然后,将试管从烘箱移除,以用肉眼观察管中的水性分散体的外观。如果观察到相分离,则从观察到的界面至水性分散体顶表面的距离被记录为“分层厚度”。如果水性分散体未示出可观察的相分离或分层厚度小于原始高度的20%,在50℃下储存28天之后,均指示没有显著的相分离,则认为存储稳定性良好。较小的分层厚度指示水性分散体的更好的存储稳定性。
DSC
在氮气气氛下,在装有自动进样器的TA Instrument DSC Q2000上,在密封铝盘中分析5-10毫克(mg)样品。通过DSC进行的Tg测量具有三个周期,包括以10℃/分钟从-60℃至150℃,接下来保持5分钟(第1周期),以10℃/分钟从150℃至-60℃(第2周期),以及以10℃/分钟从-60至150℃(第3周期)。通过“半高”方法从第3周期获得Tg。
粘合剂(PD-0)的合成
通过混合丙烯酸丁酯(1159g)、苯乙烯(404g)、丙烯酸(32.4g)、苯乙烯磺酸钠(5.8g)、甲基丙烯酸磷酸乙酯(60%活性,4g)、Silquest A-171乙烯基三甲氧基硅烷(5g,Momentive)、去离子(DI)水(406g)和89g的十二烷基苯磺酸钠(DBS)(19%固体)的水溶液,用搅拌乳化来制备单体乳液。接着,将8.8g的DBS水溶液(19%固体)和700g的DI水装入装配有机械搅拌的5升多颈烧瓶中。在氮气气氛下将烧瓶的内容物加热至90℃。向搅拌的烧瓶中添加单体乳液(53.7g)、硫酸亚铁(0.025g)和乙二胺四乙酸(EDTA)的钠盐(0.13g),接下来是过硫酸铵(APS)的溶液(5.76g的APS溶于15.6g的DI水中)。然后在120分钟内将单体乳液的剩余部分、APS的溶液(2.3g的APS溶于60g的DI水中)以及亚硫酸氢钠(SBS)的溶液(2.3g的SBS溶于63g的DI水中)添加至烧瓶中。将烧瓶温度维持在87℃。接下来,使用26g的DI水冲洗至烧瓶的乳液进料管线。冷却烧瓶内容物之后,将叔丁基过氧化氢(4.8g,70%活性)和异抗坏血酸的水溶液(2.3g的异抗坏血酸溶于63g的水中)添加至烧瓶中。烧瓶的内容物用氢氧化铵中和至pH8.0。对于冷却的批料,将TERGITOL 15-s-40表面活性剂的水溶液(11.5g的15-S-40溶于12.5g的DI水中)添加至烧瓶中,然后用5g DI水(具有40环氧乙烷的TERGITOL15-s-40脂肪醇乙氧基化物可购自陶氏化学公司)冲洗。然后将2-甲基-4-异噻唑啉-3-酮(MIT)的水溶液(3.6g的MIT溶于17.4g的DI水中)添加至烧瓶中,接下来添加0.8g的NopcoNXZ消泡剂(Nopco)。获得的粘合剂(固体:48.5%)包含苯乙烯-丙烯酸乳液聚合物,其Tg为-9℃,如通过上述DSC测量的。
水性分散体
示例(Exs)1-4、6-12和E-F和对比(Comp)示例5和13-14以及对比示例A-D的水性分散体是通过基于表1中列出的配方混合上述获得的粘合剂(PD-0)与不同类型的硅氧烷,以及可选地,按不同剂量在室温下搅拌(400rpm)20分钟制备的。
评估所获得的包括不同类型的乙烯基硅氧烷的水性分散体的稳定性,并且结果列于表1中。如表1所示,采用5.0%或更低剂量的包括环状甲基乙烯基硅氧烷或羟基封端的甲基乙烯基硅氧烷的水性分散体当在50℃下存储28天时显示出良好的稳定性(PD-1和PD-6至PD-12)。包括具有羟基端基的线性硅氧烷(PD-1)的水性分散体显示出比包含具有烷基端基的线性硅氧烷的水性分散体好得多的稳定性。当硅氧烷的剂量增加至6.0%(PD-13和PD-14)时,水性聚合物分散体的稳定性显著下降。
表1.水性分散体的组成和性质
1:基于粘合剂的固体重量,按重量计(即乳液聚合物的干重)
2:如稳定性测试中描述的在50℃存储28天之后
白色涂料组合物
基于表2中给出的配方制备两组涂料组合物样品、样品I系列和样品II系列。用于制备样品I系列和样品II系列的水分散体的类型分别在表4和表5中给出。首先,将水、Natrosol 250HBR、氨、丙二醇、OROTANTM 963、TRITON EF-106、Nopco NXZ、Ti-Pure R-706TiO2、CC-1000和CC-700混合并且在2,500rpm搅拌下研磨约30分钟以形成研磨物。然后,将粘合剂或包括粘合剂和添加剂、Tego 825、ACRYSOLTM TT-935、氨和水的水性分散体添加至研磨物中并且进一步以800rpm搅拌20分钟,以产生白色涂料组合物(OROTAN和ACRYSOL是陶氏化学公司的商标)。除非另有说明,本文所述的涂料组合物是指白色涂料组合物。根据上述测试方法评价所得涂料组合物的性质。当制备用于测试的油漆面板时,基于表3中给出的底漆组合物,根据与制备上述涂料组合物相同的程序来制备所使用的外部底漆组合物。
表2.白色涂料组合物(白色油漆)
*油漆配方的总PVC:44.14%,体积固体:44.52%,重量固体:60.78%
表3.外部底漆组合物
*CELLOSIZE、PRIMAL和KATHON是陶氏化学公司的商标。
根据上述测试方法评价所得样品I系列的涂料组合物,并且在表4中总结实验室DPUR性能的结果。如表5所示,与涂料1-B的涂料组合物相比,涂料1-E的涂料组合物显示出最低的ΔY值,即最好的DPUR性能。与涂料1-B的涂料组合物相比,添加环状甲基乙烯基硅氧烷还改进了DPUR性能。相比之下,添加四(二甲基乙烯基烷氧基)硅烷(支链硅烷)对DPUR性能(涂料1-C和涂料1-D)没有改善。
表4.样品I的配方和实验室DPUR结果
*基于粘合剂的固体重量,按重量计(即乳液聚合物的干重)
表5给出了用于制备样品II系列的涂料组合物的水性分散体的类型以及所得涂膜的DPUR和机械性质。如表5所示,包括羟基封端的甲基乙烯基硅氧烷的本发明涂料组合物提供了改进的DPUR性能,如比涂料0的低至少22%(实验室DPUR测试)或低至少16%(室外DPUR测试)的ΔY值所指示的。此外,更高的BzP荷载有助于进一步改进包括其(涂料3)的涂膜的DPUR性能。所有本发明的涂料组合物(涂料1至涂料4)提供了与涂料0的涂料组合物相当的伸长率和拉伸强度性质。
表5.样品II的配方和实验室DPUR及机械性质
1基于粘合剂的固体重量,按固体重量计的%
2室外暴露9个月后的室外DPUR
蓝色涂料组合物
将另外2%(基于每种白色涂料组合物的总重量,按重量计)的有机酞菁蓝着色剂(888-7214COLORTREND PHTHALO BLUE E)分别添加至涂料0、涂料1、涂料3和涂料4的涂料组合物中,以获得蓝色涂料0、蓝色涂料1、蓝色涂料3和蓝色涂料4。根据上述测试方法评价这些蓝色涂料组合物的室外耐久性性质。如表6所示,本发明的涂料组合物在室外暴露9个月后也显示出改进的保色性质,例如,蓝色涂料3和蓝色涂料4的蓝色油漆面板的ΔE均下降约8单位,这指示了与蓝色涂料0的相比更好的室外耐久性。
表6.室外暴露9个月后的颜色变化(蓝色油漆)
Claims (12)
1.一种水性分散体,其包括:
(a)乳液聚合物,
(b)基于所述乳液聚合物的干重,按重量计0.1%至5.5%的硅氧烷,所述硅氧烷选自线性硅氧烷、环状硅氧烷及其混合物,其中所述线性硅氧烷具有下式(I),
其中R1和R4独立地选自-OH、-NH2、-NHR5和-NR5 2,其中每个R5独立地为C1-5烷基;每个R2独立地为具有一至三个双键的C2-10直链或支链烯基;每个R3独立地选自C1-6直链或支链烷基;R23为具有1至3个双键的C2-10直链或支链烯基或C1-6直链或支链烷基;m是2至40的整数;并且n为0至20的整数;
其中所述环状硅氧烷具有下式(II),
其中每个R6独立地选自氢和C1-6直链或支链烷基;每个R7独立地为具有一至三个双键的C2-10直链或支链烯基;并且z为1至20的整数;以及
(c)基于所述乳液聚合物的干重,按重量计0至3%的光交联剂。
2.根据权利要求1所述的水性分散体,其中,在式(I)中,R1和R4独立地选自-OH和-NH2,并且m为4至16。
3.根据权利要求1所述的水性分散体,其中所述环状硅氧烷选自由四甲基四乙烯基环四硅氧烷、四乙基四乙烯基环四硅氧烷、四丙基四乙烯基环四硅氧烷、四丁基四乙烯基环四硅氧烷、四己基四乙烯基环四硅氧烷及其混合物组成的组。
4.根据权利要求1所述的水性分散体,其中所述光交联剂选自由二苯甲酮衍生物、苯并三唑衍生物、酰基氧化膦、双酰基氧化膦及其混合物组成的组。
5.根据权利要求1所述的水性分散体,其包括基于所述乳液聚合物的干重,按重量计1.0%至5.0%的硅氧烷。
6.根据权利要求1所述的水性分散体,其还包括非离子型表面活性剂。
7.根据权利要求6所述的水性分散体,其中基于所述乳液聚合物的干重,所述非离子型表面活性剂以按重量计0.1%至5%的量存在。
8.根据权利要求1所述的水性分散体,其中基于所述乳液聚合物的干重,所述光交联剂以按重量计小于0.6%的量存在。
9.根据权利要求1所述的水性分散体,其中所述乳液聚合物是丙烯酸聚合物、苯乙烯-丙烯酸聚合物或其组合。
10.根据权利要求1所述的水性分散体,其中所述乳液聚合物具有-40至10℃的Tg。
11.一种制备根据权利要求1至10中任一项所述的水性分散体的工艺,其包括:
混合乳液聚合物与基于所述乳液聚合物的干重,按重量计0.1%至5.5%的硅氧烷,所述硅氧烷选自线性硅氧烷、环状硅氧烷及其混合物;以及0至3%的光交联剂;
其中所述线性硅氧烷具有下式(I),
其中R1和R4独立地选自-OH、-NH2、-NHR5和-NR5 2,其中每个R5独立地为C1-5烷基;每个R2独立地为具有一至三个双键的C2-10直链或支链烯基;每个R3独立地为C1-6直链或支链烷基;R23为具有1至3个双键的C2-10直链或支链烯基或C1-6直链或支链烷基;m是2至40的整数;并且n为0至20的整数;
其中所述环状硅氧烷具有下式(II),
其中每个R6独立地选自氢和C1-6直链或支链烷基;每个R7独立地为具有一至三个双键的C2-10直链或支链烯基,并且z为1至20的整数。
12.一种水性涂料组合物,其包括根据权利要求1至10中任一项所述的水性分散体以及颜料和/或增量剂。
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BR112021024286A2 (pt) | 2022-01-11 |
EP3994224A4 (en) | 2023-02-01 |
WO2021000218A1 (en) | 2021-01-07 |
CA3143797A1 (en) | 2021-01-07 |
CN113939568B (zh) | 2023-12-22 |
AU2019452629A1 (en) | 2022-02-03 |
KR20220031037A (ko) | 2022-03-11 |
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